Реакция #2358485

Уравнение реакции

2-fluoro-5-(trifluoromethyl)benzaldehyde

methyl thioglycolate

potassium carbonate

DMF

→

methyl 5-(trifluoromethyl)benzo[b]thiophene-2-carboxylate

Выход 93.0%

Растворители

water

Условия реакции

Обработка

1. 1
   Температураthe reaction mixture was cooled to room temperature
2. 2
   Экстракцияextracted with tert-butyl methyl ether 3 times
3. 3
   ПромывкаThe combined organic layer was washed with water
4. 4
   СушкаThe mixture was dried over magnesium sulfate
5. 5
   Концентрированиеconcentrated under reduced pressure
6. 6
   ДругоеThe residue was recrystallized from methanol

Методика

A mixture of 5.0 g of 2-fluoro-5-(trifluoromethyl)benzaldehyde, 3.3 g of methyl thioglycolate, 4.0 g of potassium carbonate and 50 ml of DMF was stirred at 60° C. for 2 hours, and then the reaction mixture was cooled to room temperature. To the reaction mixture was added water, and extracted with tert-butyl methyl ether 3 times. The combined organic layer was washed with water, followed by saturated aqueous sodium chloride solution. The mixture was dried over magnesium sulfate, and then concentrated under reduced pressure. The residue was recrystallized from methanol to obtain 6.3 g of methyl 5-(trifluoromethyl)benzo[b]thiophene-2-carboxylate (the present compound 1).

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